CN104497575B - High-thermal-conductivity organosilicone mud and preparation method thereof - Google Patents
High-thermal-conductivity organosilicone mud and preparation method thereof Download PDFInfo
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- CN104497575B CN104497575B CN201410822370.3A CN201410822370A CN104497575B CN 104497575 B CN104497575 B CN 104497575B CN 201410822370 A CN201410822370 A CN 201410822370A CN 104497575 B CN104497575 B CN 104497575B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 46
- 229920002545 silicone oil Polymers 0.000 claims abstract description 37
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000945 filler Substances 0.000 claims abstract description 23
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 239000004014 plasticizer Substances 0.000 claims abstract description 14
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 16
- 239000003086 colorant Substances 0.000 claims description 13
- 239000012756 surface treatment agent Substances 0.000 claims description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- MJULMZZKFYNTHK-UHFFFAOYSA-N ethenyl(phenyl)silicon Chemical compound C=C[Si]C1=CC=CC=C1 MJULMZZKFYNTHK-UHFFFAOYSA-N 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229910017083 AlN Inorganic materials 0.000 claims description 3
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 230000003750 conditioning effect Effects 0.000 claims 1
- SLYCYWCVSGPDFR-UHFFFAOYSA-N octadecyltrimethoxysilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](OC)(OC)OC SLYCYWCVSGPDFR-UHFFFAOYSA-N 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000012546 transfer Methods 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract description 4
- 239000000049 pigment Substances 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000001343 alkyl silanes Chemical class 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229940116364 hard fat Drugs 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- -1 silicon lipid Chemical class 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Abstract
The invention discloses a high-thermal-conductivity organosilicone mud. The high-thermal-conductivity organosilicone mud is prepared from the following raw materials: 100 parts of silicone oil and 1000-1200 parts of heat-conducting powder filler in parts by weight, 0.5-1wt% of plasticizer and 1-3wt% of powder surface treating agent in terms of the heat-conducting powder filler, and 1-3wt% of cross-linking agent, 5-10wt% of high temperature resistant pigment and 0.01-0.015wt% of platinum catalyst in terms of the silicone oil. Besides, the invention also discloses a preparation method of the high-thermal-conductivity organosilicone mud. The high-thermal-conductivity organosilicone mud product has the advantages of high thermal conductivity, stable heat transfer property, excellent high temperature resistance, plasticity just as plasticine and the like; the preparation method of the high-thermal-conductivity organosilicone mud is simple; a better thermal-conductivity solution way can be provided for electronic heating components and radiating or other cooling devices.
Description
Technical field
The present invention relates to conduction heat transfer technical field, more particularly to a kind of organosilicon high heat conduction mud and preparation method thereof.
Background technology
Increasingly strict, the electronic product function of requiring with the fast development of Manufacturing science technology and to properties of product
The stability for using is faced with the market test of sternness, how to solve the problems, such as that equipment cooling has become the whole machine miniaturization of electronic product
The key of design.Because air conduction is poor, if the heat that equipment is generated shed not in time, local is easily formed high
Temperature, and high temperature can cause electronic component to puncture arcing etc., and then cause to damage components and parts and component, so as to affect electronic product
Reliability and normal work usage cycles.For this purpose, in the design and fabrication of electronic product, in order to chip etc. is generated heat first device
The heat that part is produced sheds, it will usually interface Heat Conduction Material is used between radiator and the components and parts of heating, with time by heat
Amount is dissipated, so as to ensure the stable normal operation of equipment.
Traditional interface Heat Conduction Material is heat-conducting silicone grease, is typically with the extremely low silicone oil of viscosity and leads to conduction powder filler
Cross mechanical strong stirring to mix, this material almost never solidifies.Heat-conducting silicone grease has excellent electrical insulating property, heat conduction
The performance such as property, high-low temperature resistant, water-fast, ozone, weather-resistant.However, because the density of conduction powder filler is far longer than silicon
The density of oil, oil meal is easily separated, therefore prior art also takes the method by being processed conduction powder filler,
To improve settlement issues, but effect is not apparent.Especially during the life-time service when temperature is more than 80 DEG C, lead
Silicone oil in hot silicone grease slowly can dissociate, and split and air inlet so as to cause thermal conductive silicon lipid layer to be dried so that heat transfer is stable
Property be deteriorated, had a strong impact on the usage cycles of electronic product equipment.
With the fast development of the whole machine miniaturization of electronic product and high-power, heat generating component temperature is constantly raised, ground
System exploitation has high thermal conductivity, stable heat transfer property, superior resistance to elevated temperatures, oil-tight, non-volatile, usage cycles length
Organosilicon heat conduction product has become the direction and emphasis studied in the industry.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of heat conductivility is stable, without permeability, use when
Between long and with good adhesion and excellent heat conducting efficiency organosilicon high heat conduction mud, be electronic heating components and parts and radiating or
More preferable heat conduction solution route is provided between other cooling devices.Another object of the present invention is to provide above-mentioned organosilicon height lead
The preparation method of warm sludge.
The purpose of the present invention is achieved by the following technical programs:
A kind of organosilicon high heat conduction mud that the present invention is provided, its raw material is consisted of:Silicone oil, conduction powder filler, plasticizer,
Surface treatment agent for powder, cross-linking agent, high temperature resistant colorant, platinum catalyst;According to parts by weight silicone oil be 100 parts, conduction powder fills out
Expect for 1000~1200 parts;In terms of conduction powder filler, plasticizer consumption be 0.5~1wt%, the consumption of surface treatment agent for powder
For 1~3wt%;In terms of silicone oil, the consumption of cross-linking agent is 1~3wt%, and the consumption of high temperature resistant colorant is 5~10wt%, platinum catalysis
The consumption of agent is 0.1~0.15wt ‰.
Further, silicone oil of the present invention is phenyl-vinyl silicon oil, and viscosity is 300~1000cp.The conductive powder
Body filler be aluminium oxide, Zinc Oxide, boron nitride, carborundum, aluminium nitride powder in one kind or its combination, its particle diameter be 0.5~
10 μm, grain shape is ball-type.The plasticizer is methyl-silicone oil, and viscosity is 100~500cp.The surface treatment agent for powder
For the one kind in long chain alkyl silane, titanate esters, hard fatty acids or its combination.The cross-linking agent is that end containing hydrogen silicone oil and side chain contain
The mixture of hydrogen silicone oil;Specially according to mol ratio end containing hydrogen silicone oil: side chain containing hydrogen silicone oil=7: 3 mixture, after compounding
Viscosity is 10~50cp, wherein, the structural formula of the end containing hydrogen silicone oil is H-Si (CH3)2-O-[Si(CH3)2-O]n-Si
(CH3)2- H, the structural formula of the side chain containing hydrogen silicone oil is C3H9-Si-O-[Si(CH3)(H)-O]n-Si-C3H9.The high temperature resistant
Colorant is cobalt blue, barba hispanica or titanium blue.The platinum catalyst is Karst platinum catalyst.
Another object of the present invention is achieved by the following technical programs:
The preparation method of the above-mentioned organosilicon high heat conduction mud that the present invention is provided, comprises the following steps:First by silicone oil with lead
Hot powder stuffing is uniformly mixed under the conditions of vacuum protection, then sequentially add in batches plasticizer, surface treatment agent for powder,
Cross-linking agent, high temperature resistant colorant, platinum catalyst, are warming up to 55~65 DEG C under the conditions of vacuum protection, react 0.5~2h, are cooled to
Room temperature obtains organosilicon high heat conduction mud finished product.
The invention has the advantages that:
(1) in inventive formulation system, silicone oil forms spatial networks crosslinking with cross-linking agent, by conduction powder filler securely
Parcel wherein, so as to ensure that resin and conduction powder filler are difficult layering, is prevented because conduction powder packing density is too big
Caused sedimentation so that product has the excellent characteristics such as oil-tight, non-volatile, storage cycle length.Also, at powder surface
Reason agent is surface-treated to conduction powder filler, eliminates powder surface such as hydroxyl or other reactive polar groups, reduces
Molecular force (such as hydrogen bond) between powder granule, is substantially increased the loading of conduction powder filler, effectively
Ensure that the high thermal conductivity of product.Additionally, by formulas optimized design, using the conduction powder filler and Nai Gao of consumption at high proportion
Warm colour material, improves the resistance to elevated temperatures of product so as under 200 DEG C of hot conditionss can with the performance of stable for extended periods of time,
Can avoid what is significantly declined similar to the heat transfer property caused by silicone oil vaporization at high temperature in prior art heat-conducting silicone grease
Problem.
(2) organosilicon high heat conduction mud of the present invention is the plasticity jelly similar to plasticine, so as to increased its construction
Method (in addition to conventional brushing and silk screen printing, can also adopt modularity), and easy construction is flexible.Meanwhile, product has
Certain elasticity, can effectively eliminate the internal stress that heat generating component is produced due to vibration, so as to ensure good heat-conducting effect, can
Play the effect such as high heat conduction, insulation, dust-proof, moistureproof, shockproof.
(3) organosilicon high heat conduction mud product of the present invention has stable, the superior heat-resisting quantity of thermal conductivity height, heat transfer property
Can, oil-tight, non-volatile and plasticity similar to plasticine the advantages of, preparation process is simple can be electronic heating unit
Between the assembling (such as radiator accessories and Led chip aluminium bases) of device and heating element and radiating or other cooling devices
More preferable heat conduction solution route is provided, can be widely applied to high power module, integrated chip, power module, auto electronic product,
The radiating of the heating elements such as controller, communication apparatus, computer and its adnexa.
Below in conjunction with embodiment, the present invention is described in further detail.
Specific embodiment
A kind of organosilicon high heat conduction mud of the embodiment of the present invention, its raw material is consisted of:Silicone oil, conduction powder filler, plasticizer,
Surface treatment agent for powder, cross-linking agent, high temperature resistant colorant, platinum catalyst.Wherein, silicone oil is phenyl-vinyl silicon oil, and viscosity is 300
~1000cp;Conduction powder filler is one kind or its group in aluminium oxide, Zinc Oxide, boron nitride, carborundum, aluminium nitride powder
Close;Plasticizer is methyl-silicone oil, and viscosity is 100~500cp;Surface treatment agent for powder is long chain alkyl silane, titanate esters, Hard Fat
One kind or its combination in fat acid;Cross-linking agent is according to mol ratio end containing hydrogen silicone oil: side chain containing hydrogen silicone oil=7: 3 mixture,
Viscosity after compounding is 10~50cp, wherein, the structural formula for holding containing hydrogen silicone oil is H-Si (CH3)2-O-[Si(CH3)2-O]n-Si
(CH3)2- H, the structural formula of side chain containing hydrogen silicone oil is C3H9-Si-O-[Si(CH3)(H)-O]n-Si-C3H9;High temperature resistant colorant is cobalt
Blue, barba hispanica or titanium blue;Platinum catalyst is Karst platinum catalyst.It is specific as follows:
Embodiment one:
1st, a kind of organosilicon high heat conduction mud of the present embodiment, its raw material is consisted of:
2nd, the preparation method of the above-mentioned organosilicon high heat conduction mud of the present embodiment, its step is as follows:
Add phenyl-vinyl silicon oil in planet machine first, conduction powder filler is sequentially added in five batches ,-
It is uniformly mixed under the conditions of the vacuum protection of 0.095MPa;Then plasticizer, surface treatment agent for powder, crosslinking are sequentially added
Agent, high temperature resistant colorant, platinum catalyst, are warming up to 65 DEG C of reaction 0.5h under the conditions of the vacuum protection of -0.095MPa, are cooled to room
Temperature obtains organosilicon high heat conduction mud finished product.
Embodiment two:
1st, a kind of organosilicon high heat conduction mud of the present embodiment, its raw material is consisted of:
2nd, the preparation method of the above-mentioned organosilicon high heat conduction mud of the present embodiment, its step is as follows:
Add phenyl-vinyl silicon oil in planet machine first, conduction powder filler is sequentially added in five batches ,-
It is uniformly mixed under the conditions of the vacuum protection of 0.095MPa;Then plasticizer, surface treatment agent for powder, crosslinking are sequentially added
Agent, high temperature resistant colorant, platinum catalyst, are warming up to 60 DEG C of reaction 1h under the conditions of the vacuum protection of -0.095MPa, are cooled to room temperature
Obtain organosilicon high heat conduction mud finished product.
Embodiment three:
1st, a kind of organosilicon high heat conduction mud of the present embodiment, its raw material is consisted of:
2nd, the preparation method of the above-mentioned organosilicon high heat conduction mud of the present embodiment, its step is as follows:
Add phenyl-vinyl silicon oil in planet machine first, conduction powder filler is sequentially added in six batches ,-
It is uniformly mixed under the conditions of the vacuum protection of 0.095MPa;Then plasticizer, surface treatment agent for powder, crosslinking are sequentially added
Agent, high temperature resistant colorant, platinum catalyst, are warming up to 55 DEG C of reaction 2h under the conditions of the vacuum protection of -0.095MPa, are cooled to room temperature
Obtain organosilicon high heat conduction mud finished product.
The physical and chemical performance index of organosilicon high heat conduction mud finished product prepared by various embodiments of the present invention is as shown in table 1 below.
The physical and chemical performance index of organosilicon high heat conduction mud finished product prepared by the various embodiments of the present invention of table 1
A kind of organosilicon high heat conduction mud of the present invention and preparation method thereof, its raw material composition and preparation method technological parameter are not
It is confined to the above-mentioned embodiment enumerated.
Claims (5)
1. a kind of organosilicon high heat conduction mud, it is characterised in that raw material is consisted of:Silicone oil, conduction powder filler, plasticizer, powder body table
Face inorganic agent, cross-linking agent, high temperature resistant colorant, platinum catalyst;According to parts by weight silicone oil be 100 parts, conduction powder filler be
1000~1200 parts;In terms of conduction powder filler, plasticizer consumption is 0.5~1wt%, and the consumption of surface treatment agent for powder is 1
~3wt%;In terms of silicone oil, the consumption of cross-linking agent is 1~3wt%, and the consumption of high temperature resistant colorant is 5~10wt%, platinum catalyst
Consumption be 0.1~0.15wt ‰;
The silicone oil is phenyl-vinyl silicon oil, and viscosity is 300~1000cp;
The surface treatment agent for powder is the one kind in octadecyl trimethoxysilane, titanate esters, hard fatty acids or its combination;
The plasticizer is methyl-silicone oil, and viscosity is 100~500cp;
The cross-linking agent is the mixture for holding containing hydrogen silicone oil and side chain containing hydrogen silicone oil, according to mol ratio end containing hydrogen silicone oil: side chain contains
Hydrogen silicone oil=7: 3 mixture, the viscosity after compounding is 10~50cp, wherein, the structural formula of the end containing hydrogen silicone oil is H-Si
(CH3)2-O-[Si(CH3)2-O]n-Si(CH3)2- H, the structural formula of the side chain containing hydrogen silicone oil is C3H9-Si-O-[Si(CH3)
(H)-O]n-Si-C3H9。
2. organosilicon high heat conduction mud according to claim 1, it is characterised in that:The conduction powder filler be aluminium oxide,
One kind or its combination in Zinc Oxide, boron nitride, carborundum, aluminium nitride powder, its particle diameter is 0.5~10 μm, and grain shape is
Ball-type.
3. organosilicon high heat conduction mud according to claim 1, it is characterised in that:The high temperature resistant colorant is cobalt blue, barba hispanica
Or titanium blue.
4. organosilicon high heat conduction mud according to claim 1, it is characterised in that:The platinum catalyst is Karst platinum catalysis
Agent.
5. the preparation method of one of claim 1-4 organosilicon high heat conduction mud, it is characterised in that comprise the following steps:First
Silicone oil is uniformly mixed with conduction powder filler under the conditions of vacuum protection, plasticizer, powder body are then sequentially added in batches
Surface conditioning agent, cross-linking agent, high temperature resistant colorant, platinum catalyst, are warming up to 55~65 DEG C, reaction 0.5 under the conditions of vacuum protection
~2h, is cooled to room temperature and obtains organosilicon high heat conduction mud finished product.
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RU2612677C2 (en) * | 2015-06-15 | 2017-03-13 | Общество с ограниченной ответственностью "Новая Химия" | Plastic silicone composition with bulk filler |
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RU2659961C1 (en) * | 2017-05-29 | 2018-07-04 | Общество с ограниченной ответственностью "Новая Химия" | Composite elastic material and method of its manufacturing |
CN107141815B (en) * | 2017-06-24 | 2020-03-24 | 肇庆皓明有机硅材料有限公司 | High-temperature-resistant low-modulus heat-conducting organosilicon material and preparation method thereof |
CN108440968A (en) * | 2018-03-27 | 2018-08-24 | 董小琳 | A kind of high heat conduction silicon aluminum nitrides rubber cushion and preparation method thereof |
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CN109401319A (en) * | 2018-09-04 | 2019-03-01 | 苏州泰吉诺新材料科技有限公司 | A kind of long-acting thermostable heat-conductive silicone grease and preparation method thereof |
CN111560187A (en) * | 2019-11-26 | 2020-08-21 | 东莞市美庆电子科技有限公司 | Heat conduction mud and preparation method thereof |
CN110903656B (en) * | 2019-11-28 | 2022-05-17 | 华南协同创新研究院 | Low-volatility temperature-resistant heat-conducting silica gel cement material and preparation method and application thereof |
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CN115404051A (en) * | 2022-09-24 | 2022-11-29 | 宁波聚力新材料科技有限公司 | High-thermal-conductivity easily-molded heat-conducting mud and preparation method thereof |
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